1

JSS MAHAVIDYAPEETHA
JSS Science and Technology University
Sri Jayachamarajendra College of Engineering
JSS Technical Institutions Campus, Mysuru – 570 006

Chemical Engineering Lab Instruction Manual

For 4th Semester B.E. degree

Department of Polymer Science and Technology

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Outcome Based Education Statements

Sri Jayachamarajendra College of Engineering
VISION: Be an international leader in engineering education, research and application of
knowledge to benefit society globally.
MISSION
M1: To synergistically develop high-quality manpower and continue to stay competitive in
tomorrow's world.
M2: To foster and maintain mutually beneficial partnerships with alumni, industry and
government through public services and collaborative research
M3: To create empowered individuals with sense of identity.

Department of Polymer Science and Technology

VISION: To excel in polymer engineering education and research and to serve as valuable
resource for multi-faceted industry and society.
MISSION
M1: To provide well balanced curriculum and conducive environment to excel in polymer and
allied engineering disciplines.
M2: Creating state-of-the-art facilities for polymer research and make the best use of the
facilities
M3: To undertake collaborative projects for long term interactions with academia and
industries.
Program Outcomes (POs) [Graduate Attributes]
Engineering Graduates will be able to:
PO1 Engineering knowledge: Apply the knowledge of mathematics, science, engineering
fundamentals, and an engineering specialization to the solution of complex engineering
problems.
PO2 Problem analysis: Identify, formulate, review research literature, and analyze complex
engineering problems reaching substantiated conclusions using first principles of mathematics,
natural sciences, and engineering sciences.
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PO3 Design/development of solutions: Design solutions for complex engineering problems and
design system components or processes that meet the specified needs with appropriate
consideration for the public health and safety, and the cultural, societal, and environmental
considerations.
PO4 Conduct investigations of complex problems: Use research-based knowledge and
research methods including design of experiments, analysis and interpretation of data, and
synthesis of the information to provide valid conclusions.
PO5 Modern tool usage: Create, select, and apply appropriate techniques, resources, and
modern engineering and IT tools including prediction and modeling to complex engineering
activities with an understanding of the limitations.
PO6 The engineer and society: Apply reasoning informed by the contextual knowledge to
assess societal, health, safety, legal and cultural issues and the consequent responsibilities
relevant to the professional engineering practice.
PO7 Environment and sustainability: Understand the impact of the professional engineering
solutions in societal and environmental contexts, and demonstrate the knowledge of, and need
for sustainable development.
PO8 Ethics: Apply ethical principles and commit to professional ethics and responsibilities and
norms of the engineering practice.
PO9 Individual and team work: Function effectively as an individual, and as a member or leader
in diverse teams, and in multidisciplinary settings.
PO10 Communication: Communicate effectively on complex engineering activities with the
engineering community and with society at large, such as, being able to comprehend and write
effective reports and design documentation, make effective presentations, and give and receive
clear instructions.
PO11 Project management and finance: Demonstrate knowledge and understanding of the
engineering and management principles and apply these to one’s own work, as a member and
leader in a team, to manage projects and in multidisciplinary environments.
PO12 Life-long learning: Recognize the need for, and have the preparation and ability to
engage in independent and life-long learning in the broadest context of technological change.
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Program Specific Outcomes (PSOs)

Graduates receiving the Bachelor of Engineering in Polymer Science and Technology will be-
PSO1: able to address the issues related to polymeric material design with the knowledge of
synthesis, structure property relationships and compounding.
PSO2: able to utilize the knowledge of polymer processing, testing, characterization, product
and mold design to produce acceptable engineering products.
PSO3: capable of taking up research/ higher education in premier institutes and employment in
polymer industries viz. rubbers, plastics, composites, adhesives, paints, etc.

Program Educational Objectives (PEOs)

PEO1: Provide graduates with strong fundamentals of science and engineering for a successful
career in Polymer Science & Technology.
PEO2: Enable graduates to pursue higher education and take up innovative research so as to
solve multidisciplinary issues.
PEO3: Equip graduates with technical skills and moral values for being responsible individuals.

Program Specific Criteria (PSCs)

PSC1: Apply chemistry, physics to understand structure, properties, rheology, processing,
performance of polymeric materials systems, for selection and design of suitable components
and process to address the concerned issues.
PSC2: Career development of members through research, consultancy and professional
activities.
PSC3: Provide collaborative learning opportunities through professional societies, industries,
institutes and alumni fraternity for promoting PST education along with professional growth of
associated individuals.
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CONTENTS
**************
Expt. No. TITTLE OF THE EXPERIMENT

1. VAPOUR – LIQUID EQUILIBRIUM

2. TRAY DRIER

3. SIMPLE DISTILLATION

4. STEAM DISTILLATION

5. PACKED BED DISTILLATION

6. FLOW THROUGH FLUIDIZED BED

7. HEAT TRANSFER IN A JACKETED VESSEL

8. HEAT TRANSFER IN A PACKED BED

9. DOUBLE PIPE HEAT EXCHANGER

10. HEAT TRANSFER THROUGH BARE AND FINNED TUBE HEAT EXCHANGER

11. SINGLE EFFECT EVAPORATOR

12. VERICAL CONDENSER

13. CALIBRATION OF THERMOCOUPLE

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EXPERIMENT 1

VAPOR-LIQUID EQUILIBRIUM
Aim: To obtain the vapor-liquid equilibrium data for the given binary system.

Apparatus: 500 ml Round bottom flask with necessary joints, a condenser, condensate collector,
specific gravity bottles.

Theory: consider a binary mixture AB in which A is more volatile. Therefore vapor pressure of
A at any temperature is greater than that of B. According to the phase rule F= C-P+2 there has to
be F= 2-2+2=2. i.e., degree of freedom for such a system is two. Thus the vapor-liquid
equilibrium between pure components A and B in a mixture is its vapor pressure-temperature
relationship. For binary mixtures, an additional variable, concentration must be considered. In
general VLE can be represented by Pxy diagram for a fixed temperature or Txy diagram for a fixed
pressure. It is customary to represent concentration in terms of mole fraction in VLE
calculations. The mole fraction of the more volatile component (A) in the liquid is designated as
x and that in the vapor phase as y*.

Procedure:
1. Take 100 ml of the given unknown mixture in a 500 ml round bottomed (RB) flask and
heat the flask over a mantle heater.
2. The vapor condenses and collects in the collecting chamber. Pour this condensate back to
the flask and continue heating for about 20 minutes and note down the boiling point. Run
off the condensate formed during this time and find its specific gravity.
3. Transfer this condensate along with the sample taken for finding specific gravity into the
RB flask with 15 ml of pure methanol.
4. Heat the RB flask again for 15 minutes and note down the boiling point. The condensate
which is collected at the end of 15 minutes is run-off to find the specific gravity.
5. Again transfer this condensate along with an additional 25 ml of pure methanol. Heat the
RB flask for 15 minutes and record the boiling point. Collect the condensate and find its
specific gravity.
 7

6. Repeat this procedure for additional 40 and 60 ml of methanol.

7. Find out the specific gravity of the original mixture.
8. Prepare a specific gravity v/s mole fraction chart.
9. Prepare Txy plot (x, y* on X-axis and T on Y-axis) for experimental values and compare
them by plotting the literature values.
10. Also report % deviation of each set of experimental x, y* with that of literature values for
corresponding temperatures.

Observations and Calculations:

1. Calibration chart:
Let A = Methanol and B = water
ρA = 0.792 g/cm³; ρB= 1.0 g/cm³

Sample Vol.of Vol. of Wt. of Wt. of Moles Moles Mole Sp.gr.

No A (ml) B (ml) A (g) B (g) of A of B fraction
of A
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Calculation of volumetric composition of methanol and water in the original mixure:

Sp.gravity of the original mixure = ……………………

Mole fraction of methanol in the original mixure, XA = …………… (from calibration chart)

VA = [ XA (MW)A]/ ρA = ………………….cm³

VB = [ XB (MW)B]/ ρB = ………………….cm³

Vt = VA + VB

Vt cm³ mixture contains VA cm³ of methanol.

100 cm³ mixture contains [VA x 100/ Vt] = ………….cm³ (say V1*)
Vol. of water in the original mixture = [100-V1*] = …………cm³ (say V2*)

Vapor – liquid equilibrium calculations:

Trial Vol. of methanol Vol. of mixture B.P (°C) Sp. gr. of the
No. added (ml) after addition (ml) condensate

5
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VLE - DATA
Trial Vol. of B, Vol. of A, Mole fraction of A Sp. gr. of Mole fraction
No. (V2) (ml) (V1) (ml) in liquid phase (x) the of A in vapor
using equation given condensate phase, (y*)
below from
calibration
chart

1 V2* V1*

2 V2* V1* + 15

3 V2* V1* + 40

4 V2* V1* + 80

5 V2* V1* + 140

[ V1 x ρA / (MW)A ]
X = ------------------------------------------------------
[ V1 x ρA / (MW)A ] + [V2 x ρB / (MW)B ]
Results :
(1) Composition of given mixture : 100 ml of given mixture contains
Methanol = ……………….ml
Water = ………………..ml
(2) VLE data for methanol water system.
T (°C)
X (Exptl.)
X (Lit.)
% Deviation
Y* (Exptl.)
Y* (Lit.)
% Deviation

(3) Plot of T (on Y-axis) Vs. x, y*(X-axis) for experimental and Literature values.
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EXPERIMENT 2

TRAY DRIER

Aim: To conduct the phenomenon of drying and to find out (a) equilibrium moisture content
(X*) and (b) critical moisture content (Xc)

Apparatus: Tray drier set up, stop-watch and thermometer.

Theory: The phenomenon of removal of relatively small amount of water or other liquids from a
solid material is called drying. This can be achieved by means of evaporationg the liquid by
direct heating (i.e. adiabatic drying where the wet solid is directly exposed to hot air) or by
indirect heating (i.e. nonadiabatic heating where the heat is transferred from an external medium
such as condensing steam through a metal surface)

Consider a bed of wet solids over which hot air is circulated. When the temperature, humidity,
velocity and direction of flow of the air across the drying surface are constant, the drying process
is said to be under constant drying conditions. The rate of water evaporated per unit area of
drying is known as the rate of drying. If the water content is above a particular level, the water
forms a film over the solid and until this film is depleted drying proceeds at a constant rate and
this period of process is called constant rate period. The driving force of heat and mass transfer
in this region is the difference in temperature. After the film disappears a concentration gradient
between the hot upper layer and the cooler lower layer with more moisture results in a slower
and a falling rate of drying. The moisture, before and after depletion of film is called bound and
unbound moisture respectively. The moisture content at the time of complete depletion of film is
called critical moisture content. The moisture content at the end of falling rate period is the
equilibrium moisture content. This is the moisture content which is in equilibrium with the
incoming air conditions and beyond this limit no more drying will occur.
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Formulae used:
Moisture content = [wt. of moisture present / wt. of dry solid] = x
Rate of drying, N = [dx. S / A dt] = -------kg/m² s
Where
A = area f drying pan in m²
S = wt. of dry sand in kg
dt = time taken for the removal of moisture content equal to dx, in seconds

Procedure:
1) Weigh out about 100 g. of given material into the pan.
2) Add 32-35 ml of water and make a uniform paste. The sand should be equally distributed
in the pan.
3) Then take the weight of sand and water in the balance provided in the drier.
4) Remove the pan from the balance and cover it with a polythene sheet so that no water
gets evaporated.
5) Switch on the blower and heater and wait till the air attains a temperature of 60°C .
6) Place the pan on the balance after removing polythene sheet.
7) Start the stop watch and note down the time required for removal of 1 g. of moisture.
8) At the same time remove 1g. weight from the balance and again note down the time for
the removal of 1 g. of moisture cumulatively.
9) Repeat the procedure until 30-31 g. of moisture is removed.
10) Find out the rate of drying and plot the graph between moisture content vs. time and rate
of drying vs. moisture content. Find out the values of critical moisture content and
equilibrium moisture content from the graph.

Observations and calculations:

Tray diameter (d) = 162 mm = ……………m
Wt. of material taken (S) = 100 g = ………. kg
Wt. of water added = ……..g = ………..kg
Area of tray (A) = [πd²/4] = ………….m²
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Sl. Wt. of Moisture dx Time dt N = [dx. S/A dt]

No moisture content, x (sec) (kg/m² s)
removed (kg)
1
2
3
4
.
.
.
.
.
.

30

Result:
Critical moisture content (Xc) = …………….
Equilibrium moisture content (X*) = ………….
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EXPERIMENT 3
SIMPLE DISTILLATION

Aim: To verify Rayleigh’s equation for the given acetone-water system.

Apparaturs: 3-necked flask, specific gravity bottle, chemical balance, water cooled condenser,
thermometer etc.

Theory:

Rayleigh’s equation is given by:

In (F/W) = [ /( ∗− )]
Distillation is the separation of constituents of a liquid mixture via partial vaporization of the
mixture and separate recovery of vapor and residue. Distiallation can be carried out by simple
methods such as flash distillation, simple or differential distillation and steam distillation or by
rectification or fractionation where only a part of the condensate is taken as product and the rest
is recycled as reflux. Flash distillation consists of vaporizing a definite fraction of the liquid in
such a way that the evolved vapor is in equilibrium with the residual liquid, separating the vapor
from the liquid and condensing the vapor.
Differential or simple distillation is considered to be made up of many steps of flash
distillation. The difference between these two is the composition in flash distillation is
equilibrium composition whereas in simple distillation equilibrium composition is obtained only
at the instant of vapor production. The process is governed by Rayleigh’s equation which is
drived based on the material balance for the system.

Let n0 moles of a binary mixture is charged to batch still. Assume that at any time during the
course of distillation, there are n moles of liquid in the still with mole fraction of the more
volatile component (A) as x and mole fraction of vapor as y* in equilibrium with the liquid. Then
the total moles of A left in the still, nA will be
nA = n x (1)
If a small amount of liquid dn is vaporized, the change in moles of component A is
y* dn = dnA (2)
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Upon differentiating equation (1), we get

dnA = n dx + x dn (3)
From (2) and (3), we get
y* dn = n dx + x dn (4)
By rearranging eq. (4), we get
dn/n = [ 1 / (y* - x ) ] dx (5)
Integrating eqn (5) between limits xw and xf, we get

= ( / )= [1/( ∗ − ) ] dx

The above equation is known as Rayleigh’s equation and is used to find out the
composition of distillate.

Notations:
F = no. of moles of feed.
W = no. of moles of residue
xf = mole fraction of more volatile component (acetone) in feed
xw = mole fraction of more volatile component (acetone) in residue
x, y* = equilibrium data for acetone-water mixture

Procedure:
(1) Take 100 ml of acetone (component A) and 100 ml of water (component B) in a distillation
flask.
(2) Set up the distillation apparatus as shown in the figure.
(3) Carry out the distillation till 90-95 ml of distillate gets collected in the receiver.
(4) See that the distillate does not get evaporated.
(5) Collect the residue and distillate.
(6) Find the volume and specific gravity of residue.
(7) Prepare mixtures of various compositions of acetone and water and find out their specific
gravities. Plot a graph of specific gravity vs.mole fraction of acetone.
 15

(8) Using the above graph find out the mole fraction of acetone in residue.
(9) Calculate the value of ln (F/W) and compare it with the area under the curve [1/(y*-x) vs. x
within limits xw and xf.

Observations and calculations

Volume of acetone = 100 ml
Volume of water = 100 ml
Volume of the feed = 100 + 100 = 200 ml
Volume of distillate = …………………….ml
Volume residue = …………………………ml
Density of acetone = 0.792 g/cm³
Wt. of empty sp. gravity bottle = W1 = ………g
Wt of empty sp. gravity bottle + water = W2 = ………g
Wt. of empty sp. gravity bottle + residue = W3 = ………g
Sp. gravity of residue = [W3 – W1 ] / [ W2 – W1 ]
Mole fraction of acetone in residue, XW can be found out from the standard graph of Sp. gravity
vs. mole fraction, corresponding to this specific gravity.

CALIBRATION CHART
Sl. Vol. of Vol. of Wt. of Wt. of Wt. of gmol gmol Mole Sp.
No water Acetone Mixture water acetone, of of fraction gravity
(ml) (ml) (g) (g) (g) water acetone of of
acetone mixture
1 10 0
2 7 3
3 6 4
4 4 6
5 2 8
6 1.5 8.5
7 1 9
8 0.5 9.5
9 0 10
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Calculation of xf:
Moles of acetone in feed = [Volume x density / mol. Wt. of acetone]
= [100 x 0.792 / 58 ] = …………….
Moles of water in feed = [Volume x density / mol. Wt of water]
= [100 x 1.0 / 18] = …….
Mole fraction of acetone in feed, xf = mole of acetone / [moles of acetone + moles of water]

(1) F = no. of moles of feed = no. of moles of acetone + no. of moles of water = ……….
(2) AMW of residue = [ xw. MW of acetone ] + [ (1- xw) MW water ]
(3) W = moles of residue = [ Volume of residue x density of residue ] / AMW
(4) Obtain the equilibrium data x Vs. y* from perry’s Hand book.

Result: Rayleigh’s equation for the given acetone-water system is verified.

"#
In (F/W) = "$
[1/( ∗ − )]!
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EXPERIMENT 4

STEAM DISTILLATION
Aim: To study the characteristics of steam distillation.
To determine the values of vaporization efficiency (ηv) and thermal efficiency (ηt) for
steam distillation of aniline

Apparatus: Distillation flask, steam generator, water cooled condenser, thermometer, separating
funnel, specific gravity bottle, measuring jar.

Theory: Steam distillation is the term applied to a batch of continuous distillation process with
open steam. The liquid is distilled by feeding open steam directly into the distillation still, so that
the steam carries with it the vapors of volatile liquid component and is then condensed to
separate the liquid from water. Steam distillation is possible only when,
1. The substance does not react with steam at the given conditions of temperature and
pressure.
2. The substance is insoluble in water.
Steam distillation method is used for the separation of high-boiling substances from non-volatile
impurities or for the removal of very high-boiling volatile impurities from still higher-boiling
substances. The process has special value where it is desired to separate substances at
temperature lower than their normal boiling points because of heat sensitivity or other reasons.
The condensed organic liquid and water do not miscible in each other. Therefore partial pressure
of each component is equal to vapor by each liquid. If P is total pressure, PA and Pw are vapor
pressure of organic liquid and water respectively. Then P = PA + PW. For ambient distillation, P
= 1 atm = 101.3 kpa. Therefore PA v/s T and (101.3 – Pw) v/s T plots intersects and this point
corresponds to distillation temperature.

Steam Requirements: Let yA and yw represent mole fraction of organic liquid and H2O
respectively in vapor phase. Then by Dalton’s law P°A = PyA= P [NA/(NA +NW)] and
P°W = Pyw = P [ NW / NA + NW ) ] where NA and NW are moles of A and W and P°A and P°W are
partial pressure of A and W.
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Therefore P°A/P°W = NA/NW = (WA/MA). We have P°A = PA and PoW=PW for steam distillation.

Therefore Ww/WA = (PW/PA). (MW/MA) (1)

Obtain PW and PA at distillation temperature from literature. The term (Ww/WA) is the amount of
open steam condensed per unit weight of liquid condensed however the actual requirement is
higher. In equation (1) vapor pressure of liquid is assumed that be equal to its partial pressure.

FORMULAE TO BE USED:

Vaporization efficiency, ηv

(wt. of aniline distilled/unit wt. of steam) actual [Ws/Ww] actual

ηv = --------------------------------------------------------- = ----------------------
(wt. of aniline distilled / unit wt. of steam) ideal [Ws/Ww ] Ideal

[Vol. of aniline in distillate x density. of aniline in distillate]

[Ws / Ww] actual = ---------------------------------------------------------------------------
[Vol. of water in distillate x density. of water in distillate]

[Ws / Ww] ideal = [Ps Ms] / [Pw Mw]

Where
Ps = Vapor pressure of aniline at distillation temperature
Pw = Vapor pressure of water at distillation temperature
Ms and Mw = Molecular weights of aniline (93.12) and water (18)

Thermal efficiency, ηt

[Distillation requirement of steam/unit wt. of sample distilled]

ηt = ------------------------------------------------------------------------------
[Actual requirement of steam / unit wt. of sample distilled]

i.e. ηt = St / Sa
where,
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(1+R) Cp,s (Td – Tr) + λs [Pw Mw]

St = -------------------------------------- + -------------------
λw + (Ts – Td ) Cp, w [ P s Ms ]

[Volume of H2O in residue x density of H2O in residue] + [volume of H2O in

distillate x density of H2O in distillate]
Sa = ---------------------------------------------------------------------------------------------------------
[volume of ANILINE in distillate x density of ANILINE in distillate ]

Wt. of aniline in residue

R = -----------------------------------
Wt. of aniline in distillate

Tr = room temperature
Td = distillation temperature
Ts = Steam temperature
Cp,s = specific heat of aniline at Td
Cp,w = specific heat of water at Td
λs = latent heat of vaporization of aniline at Td
λw = latent heat of vaporization of water at Td
Note that [λ s / λ w] = [Mw / Ms] [d(ln Pw) / d(ln Ps)]

Where, Mw and Ms are molecular weights of water and aniline respectively.

λs = [ Mw / Ms ] x [ d(ln Pw) / d ( ln Ps ) ] [λw ]

PROCEDURE:

1. Take 100 ml aniline in the distillation flask and set up the apparatus.
2. Pass the steam at a pressure of 0.25 kg/cm²
3. Note down the distillation temperature.
4. Pass the steam till about 60-70 % of the liquid distills.
5. Stop the steam and allow the residue and distillate to get cooled.
6. Using the separating funnel, separate aniline and water in residue and distillate.
7. Measure the volume of aniline and water in residue and in distillate and find out specific
gravities.
 20

8. Draw a graph of ln Pw vs ln Ps and calculate the slope. Then calculate λs.

9. Draw Hans-brandt chart [plot of (760 – Ps) vs. temperature and Pw vs. temperature) to
find out the theoritical distillation temperature and compare it with the actual value.

OBSERVATIONS AND CALULATIONS:

Volume of aniline taken = 100 ml
Distillation temperature Td = °C
Room temperature Tr = °C
Steam temperature Ts = ° C (from steam tables)
Steam pressure, P = 0.25 kg/cm² - 0.3 kg/ cm²
Cp, s = …………. (from perry’s H.B)
Cp, w = ……… (from Perry’s H.B)
λw = ………(from Perry’s H.B)
To get λs, obtain Vapor pressure data for aniline and water (from Perry’s H.B)
Then
λs= [Mw / Ms ] [d(ln Pw) / d (ln Ps ) ] x [λw]
[d(ln Pw) / d(ln Ps)] is given by slope of ln Pw Vs. ln Ps plot
Wt. of empty sp. gr. bottle = W1 = …..g
Wt. of empty sp. gr. bottle + water = W2 = ………g

Volume (ml) Wt. of sp. gr Specific

Description
Bottle + soln. (g) gravity
Water
Distilate
Aniline
Water
Resiude
Aniline

To plot ln Pw Vs. Ps graph and Hans-brandt graph, the data extracted from Perry’s Hand book is
given below.
 21

Sl. Temperature Ps Pw (P-Ps) ln Ps ln Pw

No. (ºC) (mm Hg) (mm Hg) P=760 mm Hg
1 34.8 1 41.71 759

2 57.9 5 136.08 755

3 69.4 10 223.73 750

4 82.0 20 384.90 740

5 96.7 40 674.60 720

For calculation of ηv and ηt

[ Ws / Ww ] actual
ηv = ---------------------- X 100 = ………..%
[ Ws / Ww ] ideal

ηt = [ St / Sa ] x 100 = ……………..%
(Show one specimen calculation to find out specific gravity)

Results:
For steam distillation of aniline
Vaporization efficiency, ηv = …………..%
Thermal efficiency, ηt = ………….%
 22

EXPERIMENT 5

PACKED BED DISTILLATION

Aim: To find out (a) number of transfer units (NTU) and (b) height of transfer unit (HTU) using
Fenske’s equation and Mc cabe-Thiele method under total reflux condition.

Apparatus: Packed bed column, 3- necked flask, specific gravity bottle, chemical balance, water
cooled condenser, thermometer etc.

Theory: Fractionation can be carried out in a plate column or a packed column. A packed
column is usually specified when plate devices would not be feasible because of undesirable
fluid characteristics or some special design requirement. Fractionation by means of a plate
column is stage-wise process, a discontinuos change in the composition of the components being
effected at each plate. In a packed column the liquid and vapour are in continuous countercurrent
contact and fractionation is not stagewise. Hence, the difficulty of separation to be accomplished
is best characterized in terms of transfer units rather than theoretical plates. The efficiency of
packed column is most frequently expressed in terms of height of packing to give a separation of
one transfer unit ( HTU). The height of packing to give a separation of one theoretical plate is
HETP. Under total reflux conditions, where the ratio of slop of equilibrium curve to slope of
operating line is unity, a transfer unit and a theoretical plate become identical. So in the case of
an ideal binary mixture, the packed height can be determined by finding out the number of stages
using the Mc Cabe – Thiele diagram under total reflux conditions or by using the Fenske’s
equation which gives the minimum number of stages for a specified separation (NTU). Fenske’s
equation is given a

ln xD ( 1 – xw ) / Xw ( 1 – XD)
NTU = ------------------------------------------ - 1
ln ( α avg )

where,
NTU – minimum no. of stages for the specified separation under total reflux condition.
 23

xD – mole fraction of acetone in distillate

xW – mole fraction of acetone in residue
αavg – relative volatility
Plot the Mc cabe-Thiele diagram and find out the number of stages for the specific separation.
Get the equilibrium data, x vs y for acetone-water mixture from perry’s Hand book.

Procedure:
1. Take 100 ml of water and 100 ml acetone in a round bottom flask.
2. Set up the apparatus.
3. Maintain the temperature of distillation around 55-60°C.
4. Allow the distillate to overflow for half an hour so that the vapors produced during the
distillation are completely condensed and the condensate is refluxed. This provides the
total reflux condition.
5. Collect the residue and distillate and find out their specific gravities.
6. Prepare mixtures of various compositions of acetone and water and find out their specific
gravities. Plot a graph of sp.gravity vs. mole fraction of acetone.
7. Using the above graph, find out the values of mole fractions of acetone in the residue and
distillate.
8. Calculate the values of NTU and HTU using Fenske’s equation and Mc Cabe-Thiele
method.

Observations and Calculations:

Volume of acetone = 100 ml
Volume of water = 100 ml
Room temperature = ……. °C
Distillation temperature = ……°C
Molecular weight of acetone = 58
Molecular weight of water = 18
Height of packing, Z = 43 cm
Wt. of empty sp. Gravity bottle = W1 = ….….g
Wt. of empty sp. Gravity bottle + water = W2 = ………g
 24

Wt of empty sp. Gravity bottle + mixture = W3 = ………g

Sp. gr. of mixture = [W3 – W1] / [W2 – W1]
g moles of acetone = [Volume of acetone x density ] / Molecular Weight.
Mole fraction of acetone = [ Moles of acetone ]/{[ moles of acetone] + [ moles of water]}

Calibration chart readings:

Mole
Vol. of Vol. of Wt. of Wt. of Vol. of gmol gmol Sp. gr.
Sl. fraction
Water Acetone mixture water, acetone of of of
No. of
(ml) (ml) (g.) (g.) (g.) water acetone mixture
acetone
1 10 0
2 7 3
3 6 4
4 4 6
5 2 8
6 1.5 8.5
7 1 9
8 0.5 9.5
9 0 10

Specific gravity of residue =

Specific gravity of distillate =

Vapor pressure of acetone

Relative Volatility, α = ------------------------------------
Vapor pressure of water

α1 = Relative volatility at room temperature = PA1 / PB1 = …………

α2 = Relative volatility at distillation temperature = PA2/PB2 = ……….
Where
PA2, PA2 are vapour pressure of acetone at room temperature and at distillation temperature.
PB1, PB2 are vapour pressure of water at room temperature and at distillation temperature.
αavg = [ α1 + α2 ] / 2
 25

By Fenske’s equation

ln [ xD ( 1 – xW ) / xW ( 1 – xD ) ]
NTU = ------------------------------------------ - 1
ln ( αavg )

HTU = Z/NTU

Result:

NTU HTU
By Fenkse’s equation
By Mc Cabe -Thiele method
 26

EXPERIMENT 6

FLOW THROUGH FLUIDIZED BED

Aim : (a) To observe and study the behaviour of bed during fluidization
(b) To determine the effect of velocity of fluid on pressure drop
(c) To find effect of porosity on fluid velocity
(d) To determine the minimum fluidization velocity from the experimental data and
to compare it with the value obtained from theoretical relations.

Apparatus: Fluidized bed experimental set-up, meter scale, 250 ml measuring jar, 100 ml
beaker.

Theory: Fluidization is one of the methods available for contacting granular solids with fluids.
The main advantages of fluidized bed are greater interfacial surface area of contact and high
rates of heat transfer. Fluidized beds find application in catalytic cracking, oxidation of
naphthalene to phthalic anhydride and many other chemical reactions which involves fluids and
solids. When a fluid passes upward through a bed of solids, there will be certain pressure drop
across the bed required to maintain the fluid flow. Depending upon the bed geometry, fluid
velocity and particle characteristics, the following phenomena occur with gradual increase in
fluid velocity.

At low fluid velocity, there is a pressure drop across the bed but the particles are
stationary and flow in such cases is just through a fixed bed. As the velocity is gradually
increased, a certain velocity is reached when the bed starts expanding. At this point the pressure
drop across the bed equals the mass per unit area of the bed. This point is known as
FLUIDZATION point or POINT OF ONSET OF FLUIDIZTION or INCIPIENT
FLUIDIZATION. The movement of solids at superficial velocities far below the terminal
settling velocities of the solid particles and the process correspond to a situation which is
approximately equivalent to hindered settling. The pressure drop is maximum at some point and
at this point the force exerted by fluid must not only act against the force of gravity on the
paticles but it must also overcome friction forces locking the particles together. Once the
 27

particles are separated, these forces drop off and the pressure required to maintain fluidization
becomes less. As the velocity is still further increased, the pressure drop continues to remain
constant until the bed has assumed the loosest stable form of packing. With the increase in fluid
velocity the particles separate still further from one another, the bed continues to expand, the
porosity increases but the pressure difference does not change. Particulate fluidization occurs
when the difference in density between the particles and fluid is small.

Procedure

1) Determination of initial porosity of the bed (εo)

Take the given packing material in a 100 ml beaker and note down height of bed in
the beaker. Calculate the bed volume (V1) using, V1 = C/S area of beaker X bed
height in beaker
Add water into the beaker just to fill up to bed surface. Drain out this water in to
measuring jar and note down the volume of water (V2)
Calculate initial porosity from eqn. (1) (given in next page)
2) Open the gate valve so that water enters into the column and close the valve when the
water is filled upto the full length of the bed. Note down the bed length (Lo).
3) To start the experiment, set all the manometer tappings and slowly open the gate valve.
Wait until there are no air bubbles in flow line and in manometer line.
4) Note down the manometer reading, rotameter reading and bed height.
5) Gradually increase the flow rate of water and follow step 4. Repeat the experiment for
different flow rates.
6) Continue till the bed is fluidized and finally becomes turbulent (i.e. till there is no
appreciable change in pressure drop indicated by manometer).
7) Plot ∆P/L as function of superficial velocity, and determine the minimum fluidization
velocity from the plot.
8) Plot ∆P vs. superficial velocity and porosity vs. superficial velocity.
9) Calculate minimum fluidization velocity from equation (7).
10) Report minimum fluidization velocity obtained by experiment and form theory.
 28

Equations used:
To find initial porosity, εo:
Volume of packing material = V1
Volume of water present in voids = V2
Initial porosity, εo = V2 / V1 (1)

To find porosity at any time, ε:

Initial bed height = Lo
Bed height at any time = L
Lo (1 – εo) = L (1 – ε)
OR
ε= 1 – [L0 (1 – ε0) / L]

To find superficial velocity, u: (2)

Volumetric flow rate as indicated by rotameter = Q lit./min. = Q x ( 1 x 10-3) / 60 m³/s
Superficial velocity, u = volumetric flow rate / Area of cross section of column
i.e u = Q / (πDi² / 4 ) (3)
where Di is the internal diameter of the column in meter

To calculate pressure drop, ∆P across the bed:

Manometer reading = Rm = …. cm = …..10-2 m
∆P = (ρCCl4 – ρH2O) x g x Rm ………….N/m² (4)
Where ρCCl4 = 1594 kg/m³; ρH2O = 1000 kg/m³ and g = 9.81 m/s²

To find minimum fluidization velocity, umf

From Kozney Carman equation (a special case of Ergun’s equation) we have

[∆P Dp² ε³]

------------------ = 150
L u µ (1 – ε)²
 29

At u = umf i.e., at minimum fluidization velocity

(∆P / L) DP² ε³
umf = ------------------------- (6)
150 µ (1 – ε)²

At the onset of fluidization the pressure drop across the bed equals the weight of bed per unit
area of cross section.

Let ε = εmf = Porosity at minimum fluidization condition, then from eqn. (6) we have

Dp² g ( ρP – ρH2O ) ε³mf

umf = -----------------------------------------
150 µ (1 – ε mf)

Where Dp is the diameter of the packing material (4.6 mm)

ρp is the density of glass beads (2220 kg/m3)

Observations and Calculations:

Volume of packing material taken for initial porosity measurement = V1
Volume of packing material taken for initial porosity measurement = V2
Volume of water filled into the voids = V2
Initial porosity, εo = V2/V1
Initial bed height, Lo = ……….m.
Internal diameter of the column, Di = 47 x 10-3 m
Viscosity of water at room temperature = = 1cP = 1 x 10-3 N s/m²
 30

Sl. Q Manometer reading Bed U= Porosity ∆P ∆P/L

No. LPM m³/s LLR RLR Rm Rm height Q/A, (ε) (N/m²) (N/m²
(cm) (cm) (cm) (m) L (cm) (m/s) /m)

Result:
Minimum fluidization velocity, umf (Experimental) = ……………m/s
Minimum fluidization velocity, umf (Calculated) = ………………. m/s
 31

EXPERIMENT 7
HEAT TRANSFER IN A JACKETED VESSEL

Aim: To find out the overall heat transfer coefficient.

Apparatus: Jacketed vessel, steam source, thermometers, stop watch

Theory: Heat transfer surfaces which is in the form a jacket as in the present case are often used
in the agitated vessels. When a liquid is heated in stirred tank by condensing vapor in the jacket,
the controlling resistance is usually that of the liquid in the tank. Consider a well agitated vessel
containing m kg of liquid of specific heat Cp. It contains a heat transfer surface of area A heated
by a constant temperature medium such as condensing steam at temperature Ts. If the initial
temperature of the liquid is Ta, then its temperature Tb at any time tT can be found as follows.

Rate of accumulation of energy = [energy input – energy output (=0)] (1)

For a batch of liquid with no flow in or out and no chemical reaction, eqn (1) becomes

m Cp (dT/dt) = UA (Ts – T ) + 0 (2)

Assuming U to be constant, eqn (2) can be integrated between the limits

t=0 T = Ta
t = tT T = Tb
Equation (2) can be rearranged and integrated between the limits Ta and Tb for temperature and 0
and tT for time to get the following equation

i.e., ln (Ts – Ta) / (Ts – Tb) = [U A tT / m Cp] (3)

 32

In equation (3), A, m and Cp are constants. Therefore a plot of LHS vs tT should result a straight
line with slope = (U A / m Cp). Since the values of A, m and Cp are known for the given system,
the overall heat transfer coefficient U can be evaluated.

Experimental Set-up:
The jacketed vessel essentially consists of an impeller driven by a fractional HP motor. A drain
valve is provided at the bottom of the jacketed vessel to remove the condensed steam. One more
valve is provided to drain out water from the vessel.

Procedure:
1. Fill the vessel with water and note down the height of water. Also note down the initial
temperature of the water.
2. Agitate the water at a constant speed.
3. Open the steam valve and set steam pressure at 0.5 kgf / cm².
4. Starting with a temperature (say 25°C, note down the time required for every 5 degree
rise in temperature and record times till the water temperature is about 85°C .
5. Repeat steps 1 – 4 for different steam pressure (1 kgf / cm²).
6. Tabulate the results and plot ln (Ts – Ta) / (Ts – Tb) against tT and calculate U.

Observations and Calculations:

1. Diameter of the vessel = D = 30 cm = 0.30 m
2. Height to which water is filled = h = 0.30 m
3. Mass of water taken, m = (πD² / 4) h ρH2O = …..kg.
4. Specific heat of water at constant pressure, Cp = 4.183 x 10³ J/Kg K

Trial - 1
Steam pressure = 0.5 kgf/cm² (i.e. guage pressure)
Steam temperature = Ts = …K [at Absolute pr. (= gauge pr. + Atm. Pr.)] from steam tables
Water temperature in the beginning (i.e. At t = 0), Ta = …..°C (….K).
 33

Trial -2
Steam pressure = 1 kgf / cm² (i.e. gauge pressure)
Steam temperature = Ts = ….K (at Absolute pr. (= gauge Pr. + Atm. Pr.)] from steam tables
Water temperature in the beginning (i.e. At t = 0), Ta = …..°C (….K)
Water temperature in the beginning, Ta = ….K
Steam pressure = 0.5 (or 1.0) kgf/cm²

Sl. No. Temp. Tb Temp. Tb Time, tT ln [(Ts–Ta)/ (Ts – Tb)]

(°C) (K) (seconds)

Plot ln (Ts–Ta) / (Ts – Tb) vs. tT and find out the slope. Calculate overall heat transfer
coefficient, U using the equation.

Slope. m Cp
U = ----------------------- = …………… W/m² K
A
Where A is the total heat transfer area given by
A = (πD²/4) + (πDh) = ….m²

Result :
(1) U at steam pressure ……….kgf/cm² = ……………W/m² K.
(2) U at steam pressure ………kgf/cm² =……………..W/m²K.
 34

EXPERIMENT 8
HEAT TRANSFER IN A PACKED BED

Aim: To determine the overall heat transfer coefficient and the inside heat transfer coefficients
in packed bed.

Equipment used: Packed bed heat exchanger, pressure gauge, steam source, flow meters,
thermometers.

Theory:
Solids in divided form such as powders, pellets and lumps are heated or cooled in chemical
processing for a variety of objectives such as drying, chemical reactions oxidation etc. For such
operations, solids are packed in a column and heated by a hot fluid either directly or indirectly.
If the solids are separated from the heating medium by wall as in the present case heat is
transferred by conduction.

Formulae to be used:
The rate of heat transfer between a hot and cold fluids is given by,
Q = mc Cp,c ∆Tc = U A ∆T ln (1)

Where
∆Tc = Tc2 – Tc1 (2)

And
(Th1 – Tc2 ) – ( Th2 – Tc1 )
∆ Tln = ----------------------------------------- (3)
ln [ (Th1 – Tc2 ) / (Th2 – Tc1 ) ]

The area of heat transfer is,

A = (πD²iL) (4)
For a packed tower, the individual heat transfer coefficient, hi is given by, (Reference, Perry 6th
edn. P.10 - 46)
 35

hi = 0.813 (k/Di) (Nre.P)0.9 exp (-6 Dp/Di); for (Dp / Di) < 0.35 (5)
and
hi = 0.125 (k/Di) (Nre.P)0.75 for 0.35 < (Dp/Di) < 0.60 (6)

where
NRe.P = Dp G/µ c
G = Mass flux = mc / (πD²i / 4 )
mc= Mass flow rate of cold fluid, = Vc / (60 x 10³ ) x 1000 = ………kg/s
Vc = Volumetric flow rate of cold fluid, in lit/min

Vol. flow rate in m³/s Vc (60 x 10³)

U = ---------------------------------- = ---------------------- = …..m/s
Area of c/s in m² (πD² i / 4 )

Procedure:
1. Open the inlet and outlet valves of cold water and hot water lines.
2. Maintain a constant flow rate in the inlet of cold water and hot water
3. Open the valves for steam entering the system and maintain a constant steam pressure.
4. Note down the inlet and outlet temperatures of hot and cold water.
5. Change cold water flow rate and note down the temperature readings.
6. Repeat the procedure for a different hot water flow rate.

Observations and calculations:

Length of bed = L = 1000 mm = ………m
Packed bed inner diameter = Di = 41 mm = ………m
Packed bed saddle diameter = Dp = 12 mm = ……..m
Steam pressure maintained = …………..kg/cm²
 36

Expt. Tc1, °C Tc2, °C Th1, °C Th2, °C Vc Vh

No (K) (K) (K) (K) LPM LPM
5 10
10 10
15 10
20 10

Properties Table: Take all the properties at average temperature of cold fluid.

Tc (avg) ρc Cp,c µ k
(K) (kg/m³) (J/kg K) (N s/m²) (w/m K)

mc = Mass flow rate of cold fluid = [ Vc / (60 x 10³ ) ] x 1000 = ….kg/s

Qc = mc Cp,c ∆Tc in Watts
∆Tc = Tc2 – Tc1
U = Qc / A ∆T ln
Where
A = πDi L = ……m²

(Th1 – Tc2 ) – ( Th2 – Tc1 )

∆Tln = -----------------------------------------
ln [ (Th1 – Tc2 ) / (Th2 – Tc1 ) ]

Notations:

Q (and Qc) - amount of heat transferred in watts

mc - mass flow rate of cold water in kg/s
Cp,c - Specific heat of cold water in J/Kg. K
 37

Tc1, Tc2 – Inlet and Outlet temperatures of cold water in K

U – Overall heat transfer coefficient in W/m² K
u – Velocity of fluid, m/s
A – area of heat transfer in m²
∆Tln – log mean temperature difference between the two flow streams
L – length of packed bed,m
k – Thermal conductivity of water in W/m K
NRe – Reynolds number
Dp – particle diameter of packing material, m
Di – packed bed inner diameter in meter
Vc,Vh – Volumetric flow rate of cold and hot water lit per min. (LPM)
hI – Inside heat transfer coefficient in W/m² K
G – mass flux in kg/m²s
µ - viscosity of water in N s/m²

Results:
Expt. 1 Expt. 2 Expt. 3 Expt. 4
Overall heat transfer
Coefficient,U
(w/m² K)
Inside heat transfer
coefficient, hi
(w/m² K)
 38

EXPERIMENT 9
DOUBLE PIPE HEAT EXCHANGER

Aim:

1. To find out the individual heat transfer coefficients on the hot fluid side and cold fluid
side
2. To determine the overall heat transfer coefficient.

Equipment’s required:

Double pipe heat exchanger, Steam source, Pressure gauge, Flowmeters, Thermometers, Control
valves to obtain co-current and counter current flows.

Note : In the present set-up hot fluid flows in inner tube and cold fluid in outer tube.

Theory:
In many heat transfer processes, heat is transferred from one fluid to another through a solid
wall. For e.g. tubular heat exchangers are frequently used in industry where heat transfer
between two fluid streams is desired. The exchanger symmetry, fluid property and flow rates are
the parameters forms the basis for design of heat exchangers. For a double pipe heat exchanger,
the rate of heat transfer to the cold fluid from the hot fluid is given by,
Q = Wh Cp,h ∆Th (Watts) (1)

Where

∆Tc = Tc2 – Tc1

∆ Tln = log mean temperature difference given by:

(Th1 – Tc2) – (Th2 – Tc1)

∆Tln = ------------------------------------- (2)
ln [(Th1 – Tc2)/ (Th2 – Tc1)] for counter-current flow

(Th1 – Tc2) – (Th2 – Tc2)

∆Tln = ------------------------------------- (3)
ln [(Th1 – Tc1)/ (Th2 – Tc2)] for co-current flow
 39

Individual heat transfer coefficients:

(1) Inside heat transfer coefficient (hi)
For turbulent flow: NRe = 10000 – 4,00,000, Npr = 0.7 – 120, the inside heat transfer
Coefficient is given by Dittus – Boelter equation
hi = 0.023 (kh/di)(NRe,h)0.8 (Npr,h)0.4 (4)
For laminar flow:
hi = 1.75 (kh/di)( wh C.p.h / kh L )1/3 (5)
Reynolds number and Prandtl Number for hot fluid are defined as:
NRe,h = (di uh ρh)/ µ h (6)
Npr,h = Cp,h µ h / kh (7)
Velocity of the hot fluid, uh flowing through the pipe is given by

Vol. flow rate in m³/s [(Vh / (60 x 10³)]

uh = -------------------------------- = ----------------------------- =……...m/s (8)
Area of c/s in m² (πd² i /4)

(2) Outside heat transfer coefficient (h0)

The outside heat transfer coefficient, h0 is given by
h0 = 0.023 (kc / De ) ( NRe,c) 0.81 ( NPr,c ) 0.33 (9)
where De is the equivalent diameter given by De = Di – d0.
NRe,c and NPr,c are given by equations
NRe,c = (De uc ρc)/ µ c (10)
NPr,c = Cp,c µ c / kc (11)
The velocity of the cold fluid is
Vc / (60x10³)
uc = ------------------------ =-----------------= …..m/s (12)
(πDe² / 4)

(3) The overall heat transfer co-efficient, U0

For clean tubes, the overall heat transfer co-efficient, U0 is given by the equation
1/U0 = (1/h0) + (d0/hi di ) + (xw d0 / km dln) (13)
Where dln is the log-mean diameter defined as:
dln = (d0 - di ) / [ln (d0 / di )] (14)
 40

Procedure:
1. Open the inlet outlet valves of cold water and hot water lines.
2. Maintain constant flow rates of cold and hot water by approximately opening the
corresponding valves.
3. For parallel flow (co-current flow), open valves (1) and (3) and close the valves(2) and (4)
4. Now open the steam valve and adjust the steam pressure for a constant value (>0.4 kgf/cm²)
5. Record the inlet and outlet temperatures of hot cold fluids.
6. Keeping hot water flow rate constant, change the cold water flow rate.
7. Repeat step (5) and (6) for different flow rates of cold fluid.
8. For counter current flow, open valves (2) and (4) and close the valves (1) and (3)
9. Repeat steps (2) - (7)

Observations:
Inner pipe dimension:
Outside diameter, d0 = 34 mm = ………..…..m
Inside diameter, di = 29 mm = ……………m
Wall thickness, xw = (d0 - di ) / 2 = 2.5 mm = ……m
Outer pipe dimensions:
Inside diameter, Di = 54 mm = …………….m
Thermally conductivity of the wall, km = 62.8 W/m K.
Effective length of each tube, L = 1.5 m
Number of tubes, N = 4
Steam pressure = ……………kgf / cm²

Co-current flow:

Expt. Tc1, °C Tc2, °C Th1, °C Th2, °C Vc Vh

No. (K) (K) (K) (K) LPM LPM
1 10 10
2 12.5 10
3 15 10
 41

Counter-current flow:

Expt. Tc1, °C Tc2, °C Th1, °C Th2, °C Vc Vh

No. (K) (K) (K) (K) LPM LPM
1 10 10
2 12.5 10
3 15 10

Specimen calculations:
Note: All the properties like ρh, µ h, kh and Cp,h are to be taken at the average fluid temperature.
1. Calculate mass flow rate of hot fluid in kg/s = Wh = [Vh / (60x10³ )] x ρh
2. Calculate mass flow rate of cold fluid in kg/s = Wc = [Vc / (60x10³ )] x ρc
3. Calculate ∆Tln from eqn. (2) or eqn. (3)
4. Calculate Q from eqn. (1), i.e. Q = Wh Cp,h ∆Th (in Watts)
5. Area of heat transfer, A = πdi L N = π x ( 29 x 10-3 ) x 1.5 x 4 = 0.5466 m²
6. Overall heat transfer coefficient , U = Q / (A ∆Tln )
7. Calculate uh from eqn. (8).
8. Compute NRe,h and NPr,h from eqns (6) and (7)
9. Compute hi from eqn. (4) or from eqn. (5) based on NRe range
10. Calculate NRe,c and NPr,c from eqns. (10) and (11)
11. Calculate velocity of cold fluid using eqn. (12)
12. Calculate h0 from eqn. (9) and dln from equation (14).
13. Calculate overall heat transfer coefficient for a clean tube, U0 from eqn. (13)
 42

Properties Table: Take all the properties at average fluid temperature.

COLD FLUID
Tc (avg) = ρc Cp,c µc kc
[ Tc1 + Tc2 ] / 2 (kg/m³) (J/kg k) (N s/m²) (w/m k)
(k)
Co - current

Counter- current

HOT FLUID

Tc (avg) = ρh, Cp,h µh kh

[ Th1 + Th2 ]/2 (kg/m³) (J/kg k) (N s/m²) (w/m k)
K
Co - current

Counter- current
 43

Notations:
A - Area of heat transfer
Cp,h - Specific heat of hot water in J/kg K
Cp,c - Specific heat of cold water in J/Kg K
di - Internal diameter of inside tube, m
Di - Internal diameter of outside tube, m
d0 - Outer diameter of inside tube, m
hi - inside heat transfer coefficient in W/m² K
kh - Thermal conductivity of hot fluid in W/m K
kc - Thermal conductivity of cold fluid in W/m K
km - Thermal conductivity of wall in W/m K
L - Effective length of each tube (=1.5m)
N - Number of tubes (=4)
Q – Rate of Heat Transfer
Th1, Th2 - Inlet and outlet temperatures of hot fluid in K
Tc1, Tc2 - Inlet and outlet temperatures of cold fluid in K
U0 - Overall heat transfer coefficient in W/m² K
uc, uh - Velocity of cold and hot fluid , m/s
Vc, Vh - Volumetric flow rate of cold and hot fluid, lpm
Wc, Wh - Mass flow rate of cold and hot fluid, kg/s
Xw - Thickness of wall, m
ρc, ρh - Densities of cold and hot fluid, kg/m3
µ c, µ h - Viscosities of cold and hot fluid, Ns/m2

RESULT:
Co-current flow
Expt. No. Q (m3/s) U0 (w/m² k) hi (w/m² k) h0 (w/m² k)

Counter-current flow
Expt. No. Q (m3/s) U0 (w/m² k) hi (w/m² k) h0 (w/m² k)
 44

EXPERIMENT 10
HEAT TRANSFER THROUGH BARE AND FINNED TUBE HEAT EXCHANGERS

Aim: To determine: (i) Overall heat transfer coefficient, U

(ii) Air side heat transfer coefficient, ha
(iii) Fin efficiency

Apparatus: Bare and Finned tube heat exchanger set up, steam source, pressure gauges, beakers.

Theory: Difficult heat exchange problems occur when of two fluid streams has a much lower
heat-transfer coefficient than the other. A typical case is heating a fixed gas, such as air by means
of condensing steam. The individual coefficient for the steam is typically 100-200 times that for
the air stream, consequently, the overall heat transfer coefficient is essentially equal to the
individual coefficient for the air, resulting a low capacity of unit area of heating surface. As a
result tube length required is increased considerably to provide reasonable capacity. To conserve
space and to reduce the cost of equipment in these cases, extended surfaces may be used in the
form of fins, pegs, disks and other appendages thereby the outside area is multiplied several
times. The fluid stream having low coefficient (eg. air) is brought into contact with the extended
surface and flows outside the tubes, while the other fluid having the high coefficient flows
through the tubes. Fin efficiency is defined as the ratio of mean temperatures difference from
surface to fluid divided by the temperatures difference from fin to fluid at the base or root of the
fin.

Procedure:

1. Fill a bucket with cold water (to approx. half the volume) and note down the weight.
2. Drain out the residual water in bare and finned tube by opening taps at the bottom.
3. Close the taps.
4. Close the top valve of bare and finned tube heat exchanger and open the main line steam
valve.
 45

5. Set steam pressure to 1 kg/cm² in bare and finned tube by appropriately opening the top
valve.
6. Collect the condensate from both the heat exchangers for 5 minutes. (This can be done by
fixing a rubber tube to stream trap and injecting the discharge to the cold water in buckets
for known time.)
7. Weigh the buckets and calculate the weight gain. From this, find out condensate flow
rate.
8. Repeat the experiment for 0.5 kg/cm² pressure of steam.

Formulae used:
1. Q = m λ …..Watts (1)
Where m = mass flow rate of condensate kg/s
λ= Latent heat vaporization J/Kg

2. U = Q/[A (Ts –Ta )] ……W/m² K (2)

Where Ts = steam temperature
Ta = Ambient temperature

3. Npr = Cp µ / k (3)
Where Cp = Specific heat (J/Kg K), k = Thermal conductivity (W/m k) and
µ = Viscosity of the fluid (Ns/m²) [Note: Cp µ and k corresponds to those of air at avg.
temp. = (Ts + Ta )/2 ]

βg (Ts – Ta ) L³ ρ²air
4. NGr = ----------------------------- (4)
µ²

ρair at Ta - ρair at Ts
where, β = -----------------------------------
[ρair at (Ts + Ta ) /2 ] x (Ts - Ta)

5. ha = 0.13 [NGr Npr ] 1/3 (k/L ) W/m² K. (5)

if (NGr. Npr) is > 109 (Refer Mc Cabe smith)
 46

OR

6. ha = 0.59 [ NGr NPr ] ¼ (k/L) W/m² K. (6)

4 9
if (NGr. NPr ) is between 10 - 10
(Note: k = thermal conductivity of air and L = 25 mm = 25x10-3 m)

tan h (mL)
7. Efficiency = ---------------------- x 100 (7)
mL

ha P
where, m = ---------------- (8)
kf Af

kf = Thermal conductivity of the wall, 62.8 w/m k

P = Perimeter of fin = 2 (bf + t)
Af = (Area of fin) = bf x t
t = Thickness of fin = 3mm
bf = Breadth of fin = 1500 mm

Observations:
N = Number of fins = 12
Lf = Length of the fin = 25mm
D0 = Outside dia. = 84 mm
Di = Inner dia. = 78 mm

Gauge Pressure Weight of the condensate Mass flow rate of the

(kg/cm²) collected (kg) condensate (kg/s)
In fin tube In bare tube In fin tube In bare tube
(mfin) (mbare)
1.0
0.5
 47

Properties Table:

Ambient temp, Ta = ….°C = …..K

Gauge Steam Avg. λs ρair at Ta ρair at Ts ρair at µair kair Cp of air
Pressure Temp. Temp (J/kg) (kg/m3) (kg/m3) (Ts+Ta)/2 (Ns/m²) (w/mk) (J/kg k)
(kg/cm²) Ts (k) Tavg(k) (kg/m3)

Specimen Calculations:
Afin = πD0 bf + 2 lf bf N = ………….
Abare = πD0bf
Qbare = mbare λ
Qfin = mfin λ
Ufin = ………; Ubare = …………….. (from eqn.2)
Npr. = ……….. (from eqn.3)
β and NGr = ………… (from eqn.4)
ha = ……………. (from eqn.5)
Density of air = PM/RT, P =1 atm, M = avg. MW of air = [(0.79 x 28) + (0.21 x 32)]
R = 0.08026 atm.m3/kg.K (for air density calculation)

RESULT:
Experiment 1 Experiment 2
Steam pressure = …… Steam pressure = ……
Overall heat transfer
coefficient, U
(w/m2k)
Air side heat transfer
coefficient, ha
(w/m2k)
Fin efficiency, ηf (%)
 48

EXPERIMENT 11
SINGLE EFFECT EVAPORATOR

Aim: To calculate the heat balance and mass balance over a single effect evaporator.

Apparatus: Sinlge effect evaporator set-up, Steam supply, bucket, weighing scale, necessary
reagents and glass-wares for titration.

Procedure:
1. Prepare a dilute solution of sodium chloride or sodium carbonate and fill it in the feed
tank. Find out its concentration by titration.
2. Send the dilute feed solution into the evaporator at a particular constant flow rate and
note down the rotameter reading. This flow rate should be preferably low, and it should
be maintained constant.
3. Let in the steam and adjust the steam pressure to a required pressure to a required value,
say 0.2 kg/cm² (gauge). It should be maintained constant.
4. Collect the concentrated liquor continuously at the bottom and measure its flow rate.
5. Collect the steam condensate in a bucket and measure its flow rate.
6. Adjust a suitable flow rate of cooling water to the condenser and note down the flow rate
of the overhead vapors condensed.
7. Allow the system to reach steady-state. It may take 60-90 minutes. All the flow rate
should remain constant.
8. When the system attains steady-state note down the following.
a) Feed temperature
b) Feed flow rate
c) Conc. Liquor flow rate and temperature
d) Flow rate of steam condensate
e) Flow rate of overhead vapors condensed.
f) Steam pressure and temp.
9. Collect a sample of concentrate liquor and find out its concentration by titration.
10. Using these observations, mass balance and heat balance calculations can be done.
Formulas to be used and tabular column (To be worked out)
 49

EXPERIMENT 12
VERTICAL CONDENSER

Aim: To determine
i) Overall heat transfer coefficient, U
ii) Steam side film coefficient, hs
iii) Cold fluid side heat transfer coefficient, hi
iv) To draw Wilson’s plot and hence calculate the value of hs

Apparatus: The unit is as shown in the figure. It consists of ¼” G. I pipe inside which passes a
copper pipe. Cold water flows in the copper pipe steam in ¾” G.I pipe. The unit is completely
insulated by asbestos rope and covered by aluminum sheet and mounted on angle iron frame. It
is provided with vent, steam valve, pressure gage, steam trap, cold water inlet valve, thermowell
at inlet and outlet of cold water.

Procedure:
Allow cold fluid to flow through the condenser, adjust steam pressure and allow the inlet and
outlet temperatures of cold fluid to come to steady values. After the steady state has been
reached, note down, the inlet and outlet temperature, of cold fluid flow rate of cold fluid and the
steam pressure, also note down the time taken for 2cm. Rise in condensate level in the collector.
Keeping the steam pressure constant, take minimum 10 readings for different clod fluid flow
rates. For another set of observation change the steam pressure and repeat all the steps followed
earlier.

Calculations:
A)

For 200<Re<2000
B)
Plot 1/U Vs 1/v from the values of the intercept hs can be calculated.
 50

Readings to be taken:

Steam pressure Cold water Cold water temperature Time taken

Flow rate Inlet temp. Outlet temp.

Results: Overall transfer coefficient, U =

Steam side heat transfer coefficient, hs (calculated) =
Inside heat transfer coefficient, hi =
Steam side heat transfer coefficient, hs (from wilson’s plot) =
 51

EXPERIMENT 13
CALIBRATION OF THERMOCOUPLE

Aim: To compare the given K-type thermocouple with a standard thermometer.

Apparatus: K-type thermocouple, Milli-Voltmeter, Heating mantle, conical flask, thermometer,

thermometer socket.

Theory:
A thermocouple is a sensor for measuring temperature. It consists of two dissimilar metals,
joined together at one end, which produce a small unique voltage at a given temperature. This
voltage is measured and interpreted by a thermocouple. K-type thermocouple is made up of
chromel as positive wire and alumel as negative wire. Chromel is an alloy containing 90%
chromium, 10% nickel, 2% Al and 2% Al and 2% S and Mg. This type of thermocouple is
suitable for the temperature range of 200 to +1200°C. The basic thermoelectric laws are:

i) Seebeck effect
States that when two dissimilar metal wires are connected with each in a loop to form two
junctions, maintained at 2 different temperatures, a voltage potential or EMF will be generated
and the current will be proportional to the difference in potential between the junctions and the
metals used. The higher the temperature difference, the higher is the emf and current in the loop.
The magnitude of the EMF is in the order of few millivolts.

ii) Peltier Effect

States that when a current flow across the junction of two metals, heat is absorbed at the junction
when the current flows in one direction and liberated if the current is reversed. The amount of
heat liberated if the current is reversed. The amount of heat liberated if or absorbed is
proportional to the quantity of electricity which crosses the junction and the amount liberated or
absorbed. When unit current passes through unit time it is called Peltier effect.
 52

Procedure:
1. Fill a conical flask with water to half and place a thermometer socket inside the flask.
2. Put few drops of paraffin liquid into the thermometer socket for good thermal contact.
3. Insert the thermocouple one junction and thermometer into the thermometer socket.
4. Keep the conical flask assembly on a heating mantle.
5. Connect the other end of thermocouple to the digital multimeter and set the multimeter to
read DC voltage in millivolts.
6. Note down the room temperature using thermometer and corresponding mV (ERM) from the
table.
7. Turn on the heating mantle by switching the mains.
8. Note down the digital multimeter reading in mV for every 5 ºC rise in bath temperature
(TB) of thermometer.
9. As mentioned in the theory, the multimeter reading corresponds to the difference in
temperature between the room temperature and water batch. To calibrate the thermocouple,
we have to take the room temperature into consideration to get absolute value of
temperature measured. Find the equivalent millivolt value (ERM) for the room temperature
from the corresponding thermocouple table. Then add this millivolt value (corresponding to
the room temperature) to every multimeter reading (EMM) and tabulate the values.
10. Calculate the error using the relation given below.
11. Plot the graph of E (on X axis) v/s TB and TB v/s TTC.

Observation:
Room temperature = ……………..ºC
Corresponding mV from table, ERM =………………..mV

Calculation:
% Error = [(TB – TTC) / TB] X 100
 53

Temperature % Error
Temperature of bath Multimeter Total EMF
Serial corresponding
(from thermometer) reading, E=EMM+ERM
No. to E from table,
TB (°C) EMM (mV) (mV)
TTC (ºC)

Report: Error ……………% to ………..%

 54

TABLE FOR K-TYPE THEMOCOUPLE

Thermoelectric voltage in mV
0 1 2 3 4 5 6 7 8 9
°C
0 0.000 0.039 0.079 0.119 0.158 0.198 0.238 0.277 0.317 0.357
10 0.397 0.437 0.477 0.517 0.557 0.597 0.637 0.677 0.718 0.758
20 0.798 0.838 0.879 0.919 0.96 1.00 1.041 1.081 1.122 1.163
30 1.203 1.244 1.285 1.326 1.366 1.407 1.448 1.489 1.530 1.571
40 1.612 1.653 1.694 1.735 1.776 1.817 1.858 1.899 1.941 1.982
50 2.023 2.064 2.106 2.147 2.188 2.230 2.271 2.312 2.354 2.395
60 2.346 2.478 2.519 2.561 2.602 2.644 2.685 2.727 2.768 2.810
70 2.851 2.893 2.934 2.976 3.017 3.059 3.100 3.142 3.184 3.225
80 3.267 3.308 3.350 3.391 3.433 3.474 3.516 3.557 3.599 3.640
90 3.682 3.723 3.765 3.806 3.848 3.889 3.931 3.972 4.013 4.055
100 4.096 4.138 4.179 4.220 4.262 4.303 4.344 4.385 4.427 4.468
110 4.509 4.550 4.591 4.633 4.674 4.715 4.756 4.797 4.838 4.879
120 4.920 4.961 5.002 5.043 5.084 5.124 5.165 5.206 5.247 5.288
130 5.328 5.369 5.410 5.450 5.491 5.532 5.572 5.613 5.653 5.694
140 5.735 5.775 5.815 5.856 5.896 5.937 5.977 6.017 6.058 6.098
150 6.318 6.179 6.219 6.259 6.299 6.339 6.380 6.420 6.460 6.500
160 6.540 6.580 6.620 6.660 6.701 6.741 6.781 6.821 6.861 6.901
170 6.941 6.981 7.021 7.060 7.100 7.140 7.180 7.220 7.260 7.300
180 7.340 7.380 7.420 7.460 7.500 7.540 7.579 7.619 7.659 7.699
190 7.739 7.779 7.819 7.859 7.899 7.939 7.979 8.019 8.059 8.099
200 8.138 8.178 8.218 8.258 8.298 8.338 8.378 8.418 8.458 8.499
 55

Question Bank
1. List the various modes of heat and mass transfer.
2. Mention the SI units of heat and mass flux.
3. Define conduction and write the governing equation.
4. Write the SI unit of thermal conductivity (k).
5. Write the SI unit of convective heat transfer coefficient (h).
6. Convert 100 cal to Joules.
7. Convert 100 °C to Kelvin.
8. Convert 100 PSI to atm.
9. Convert 100 LPM to m3/s.
10. Define specific heat and write its SI unit.
11. Distinguish between drying and evaporation.
12. Define critical and equilibrium moisture content.
13. Define bound and unbound moisture.
14. How do you ensure constant rate of drying?
15. Write the phase rule and explain each term.
16. Define mole and mole fraction.
17. How do you generate VLE data experimentally?
18. What does ‘x’ and ‘y∗’ indicates in VLE experiment?
19. Define specific gravity and write its value for water and methanol.
20. Define distillation and list the various types of distillation.
21. Mention the principle of distillation process.
22. Write the governing equation for simple distillation.
23. What does ‘Xf’ and ‘Xw’ indicates in simple distillation.
24. Write the boiling point diagram and show the bubble point and dew point curve.
25. What is the use of calibration chart in mass transfer experiments?
26. What are the prerequisites to conduct steam distillation?
27. What are the applications of steam distillation?
28. Define vapor pressure and partial pressure.
29. Define sensible and latent heat.
30. Define latent heat of vaporization and give its SI unit.
 56

31. Define reflux and why refluxing is done?

32. List some of the packing materials used in distillation.
33. Define relative volatility and what does its value signifies?
34. Relate NTU and HTU.
35. Define steady and unsteady state heat transfer.
36. How do you estimate steam temperature?
37. Define LMTD for co-current and counter current flow.
38. Write the temperature-length curve for co-current and counter current flow heat
exchangers.
39. Why all parameter values taken at a mean temperature?
40. Write the SI unit of overall heat transfer coefficient.
41. Define Reynolds and Prandtl numbers.
42. Define Nusselt number.
43. Write the Dittus-Boelter equation.
44. List the various types of heat exchangers.
45. Define fin efficiency.
46. Define effectiveness of a fin.
47. Write the expression for Grashof’s number.
48. What is the need of extended surface heat exchangers.
49. Compare between a thermometer and a thermocouple.
50. What is the principle of thermocouple?
51. List the various types of thermocouples.
52. Mention the alloys and its composition used in K-type thermocouple.
53. State the Seebeck effect.
54. List the characteristics of thermometer fluid and give few examples for the same.
55. Define Biot number and mention its significance.
56. Write the density value of water in SI and CGS units.
57. Calculate the molecular weight of air.
58. Give the SI unit of viscosity.
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Work sheet
 58

Work sheet